Method for preparing tris(trialkylsilane)phosphate

Abstract

The present invention relates to the technical field of compound preparation, specifically disclosing a method for preparing tris(trialkylsilane)phosphate. The method comprises the following steps: reacting a trialkylsilanol salt represented by Chemical Formula 1 with a phosphorus oxyhalide represented by Chemical Formula 2 in a non-aqueous solvent at a molar ratio of (3.05-3.2):1 at 100°C-200°C and 0.6MPa-1.5MPa to produce tris(trialkylsilane)phosphate. The method has a simple process route, high reaction conversion rate, high product purity, and simple post-processing.

Description

Technical Field

[0001] The present invention relates to the technical field of compound preparation, and in particular to a method for preparing tris(trialkylsilane)phosphate. Background Art

[0002] Tris(trialkylsilane)phosphates, such as tris(trimethylsilane)phosphate, can be used as electrolyte additives for lithium-ion batteries. Electrolytes containing these additives can form a low-resistance coating on the negative electrode surface without compromising the battery's high-current performance, significantly suppressing self-discharge and improving cycle performance. Batteries containing these electrolytes can be used as power batteries in electric vehicles. Various methods for preparing tris(trialkylsilane)phosphates have been reported, but these methods currently suffer from issues such as low reaction conversion rates and low product purity. Summary of the Invention

[0003] The present invention aims to solve at least one of the technical problems in the related art to a certain extent. To this end, the present invention aims to provide a new method for preparing tris(trialkylsilane)phosphate, which has a high reaction conversion rate, a high product purity, and simple post-processing.

[0004] Specifically, the present invention provides a method for preparing tris(trialkylsilane)phosphate, comprising the following steps:

[0005] At 100°C-200°C and 0.6MPa-1.5MPa, a trialkylsilicon alkoxide represented by Chemical Formula 1 and a trihalogenated phosphorus represented by Chemical Formula 2 are reacted in a non-aqueous solvent at a molar ratio of (3.05-3.2):1 to generate tris(trialkylsilane)phosphate.

[0006] Chemical formula 1

[0007]

[0008] Chemical formula 2

[0009]

[0010] in,

[0011] R is selected from C1-C6 alkyl;

[0012] M is selected from any one of lithium, sodium and potassium;

[0013] X is selected from any one of fluorine, chlorine and bromine.

[0014] The invention adopts trialkylsilicon alkoxide and trihalogenated phosphorus as reaction raw materials, and generates tri(trialkylsilane)phosphate by reaction under heating and pressure. The process route is simple, the reaction conversion rate is high, the product purity is high, and the post-processing is simple.

[0015] According to some embodiments of the present invention, R is selected from C1-C4 alkyl.

[0016] According to some embodiments of the present invention, R is selected from any one of methyl and ethyl.

[0017] According to some embodiments of the invention, X is selected from fluorine.

[0018] According to some embodiments of the present invention, the reaction temperature is 140° C.-170° C., the reaction pressure is 0.8 MPa-1.2 MPa, and the reaction time is 2 h-15 h.

[0019] According to some embodiments of the present invention, the non-aqueous solvent includes one or more of dichloromethane, dichloroethane, ethyl acetate, acetonitrile, diethyl ether, ethylene glycol dimethyl ether, and dimethyl carbonate.

[0020] According to some embodiments of the present invention, the water content of the non-aqueous solvent is below 50 ppm.

[0021] According to some embodiments of the present invention, the reaction is carried out in an anhydrous atmosphere.

[0022] According to some embodiments of the present invention, after the reaction is completed, the method further comprises post-processing the obtained reaction solution; the post-processing comprises filtration and vacuum distillation; the vacuum distillation temperature is 10°C-180°C, and the pressure is -0.098MPa ~ 0.098MPa; preferably, the vacuum distillation temperature is 150°C-170°C, and the pressure is -0.098MPa ~ -0.09MPa.

[0023] According to some embodiments of the present invention, reacting a trialkylsilicon alkoxide with a phosphorus oxyhalide in a non-aqueous solvent includes: dissolving the trialkylsilicon alkoxide in the non-aqueous solvent to obtain a mixed solution; and adding the phosphorus oxyhalide to the mixed solution.

[0024] Additional aspects and advantages of the present invention will be set forth in part in the description which follows and, in part, will be obvious from the description which follows, or may be learned by practice of the present invention. BRIEF DESCRIPTION OF THE DRAWINGS

[0025] Figure 1 This is the phosphorus spectrum of tris(trimethylsilyl)phosphate prepared in Example 1.

[0026] Figure 2 This is the phosphorus spectrum of tris(triethylsilyl)phosphate prepared in Example 6. DETAILED DESCRIPTION

[0027] The embodiments of the present invention are described in detail below. The embodiments described below are exemplary and are only used to explain the present invention, and should not be understood as limiting the present invention.

[0028] In the description of the present invention, unless otherwise specified, "plurality" means two or more. "Multiple" means two or more. As used herein, the terms "comprising" or "including" are open-ended expressions, meaning they include the contents specified in the present invention but do not exclude other aspects.

[0029] The endpoints of the ranges and any values ​​disclosed herein are not limited to the precise ranges or values, and these ranges or values ​​should be understood to include values ​​close to these ranges or values. For numerical ranges, the endpoints of each range, the endpoints of each range and individual point values, and the individual point values ​​can be combined with each other to obtain one or more new numerical ranges, which should be considered to be specifically disclosed herein.

[0030] Tris(trialkylsilane)phosphates, such as tris(trimethylsilane)phosphate, can be used as electrolyte additives for lithium-ion batteries. Electrolytes containing these additives can form a low-resistance coating on the negative electrode surface without compromising the battery's high-current performance, significantly suppressing self-discharge and improving cycle performance. Batteries containing these electrolytes can be used as power batteries in electric vehicles. Various methods for preparing tris(trialkylsilane)phosphates have been reported, but these methods currently suffer from issues such as low reaction conversion rates and low product purity.

[0031] To solve the above problems, the present invention proposes a new method for preparing tri(trialkylsilane)phosphate. The method uses trialkylsilane alkoxide and trihalogenated phosphorus as reaction raw materials, and reacts under heating and pressure to produce tri(trialkylsilane)phosphate. The process route is simple, the reaction conversion rate is high, the product purity is high, and the post-processing is simple.

[0032] Specifically, the present invention provides a method for preparing tris(trialkylsilane)phosphate, comprising the following steps:

[0033] At 100-200° C. and 0.6-1.5 MPa, a trialkylsilicon alkoxide represented by Chemical Formula 1 and a trihalogen phosphorus oxyhalide represented by Chemical Formula 2 are reacted in a non-aqueous solvent at a molar ratio of (3.05-3.2):1 to generate tris(trialkylsilane)phosphate.

[0034] Chemical formula 1

[0035]

[0036] Chemical formula 2

[0037]

[0038] in,

[0039] R is selected from C1-C6 alkyl;

[0040] M is selected from any one of lithium, sodium and potassium;

[0041] X is selected from any one of fluorine, chlorine and bromine.

[0042] The reaction scheme of the above reaction is as follows:

[0043] .

[0044] This reaction has high requirements for water content, and both the raw materials and the product are prone to hydrolysis, so the water content in the reaction system needs to be strictly controlled. Therefore, the present invention adopts anhydrous solvent for the reaction.

[0045] Trialkylsiliconates are strongly alkaline reagents, or nucleophiles, and phosphorus oxyhalides are acidic gases, or electrophiles. The two react readily and rapidly. By maintaining high reaction temperature and pressure, and controlling the feed ratio, trialkylsiloxy groups can completely replace the halogen atoms in the phosphorus oxyhalide, forming tris(trialkylsilane)phosphate.

[0046] In some embodiments, the reaction temperature can be 100°C, 110°C, 120°C, 130°C, 140°C, 150°C, 160°C, 170°C, 180°C, 190°C, or 200°C.

[0047] In some embodiments, the reaction pressure can be 0.6 MPa, 0.7 MPa, 0.8 MPa, 0.9 MPa, 1.0 MPa, 1.1 MPa, 1.2 MPa, 1.3 MPa, 1.4 MPa, or 1.5 MPa.

[0048] A 5% to 20% excess of trialkylsilicon alkoxide ensures complete reaction of the POF3 gas without the formation of intermediates such as difluorosilicon phosphate, thereby improving product purity. In some specific embodiments, the molar ratio of trialkylsilicon alkoxide to phosphorus oxyhalide can be 3.05:1, 3.1:1, 3.15:1, or 3.2:1.

[0049] In some embodiments, R is selected from C1-C4 alkyl. Shorter alkyl chains are beneficial for increasing collision contact of reaction sites, thereby improving reaction conversion rate and product purity.

[0050] In the present invention, "C1-C6 alkyl" refers to a linear or branched alkyl group having 1 to 6 carbon atoms, preferably a linear or branched alkyl group having 1 to 4 carbon atoms. Examples of alkyl groups include methyl, ethyl, n-propyl, isopropyl, n-butyl, sec-butyl, isobutyl, tert-butyl, n-pentyl, and n-hexyl. The C1-C6 alkyl group is preferably methyl, ethyl, n-propyl, isopropyl, n-butyl, sec-butyl, isobutyl, and tert-butyl.

[0051] In some embodiments, R is selected from any one of methyl and ethyl. Trimethylsiliconate and triethylsiliconate readily react with phosphorus oxyhalides, particularly phosphorus oxytrifluoride, thereby improving reaction conversion and product purity.

[0052] In some embodiments, X is selected from fluorine. Phosphorus oxytrifluoride has a higher reactivity, is more conducive to the formation of the target product, has fewer by-products, and has a high product purity. When using phosphorus oxytrifluoride as a raw material, the higher the reaction temperature and pressure, the shorter the reaction time, and the faster the reaction rate. This is because phosphorus oxytrifluoride is a gas, and increasing the pressure increases the concentration of gas molecules. Moreover, under high pressure, the distance between molecules decreases, and the collision frequency increases, which accelerates the reaction rate.

[0053] In some embodiments, R is selected from any of methyl and ethyl; M is selected from any of lithium, sodium, and potassium; and X is selected from fluorine. Sodium trimethylsiliconate or sodium triethylsiliconate reacts rapidly with phosphorus oxyfluoride under anhydrous conditions, under heating and pressure, to produce tris(trimethylsilyl)phosphate or tris(triethylsilyl)phosphate with high gas chromatographic purity. The desired product can be obtained after simple post-processing.

[0054] In some specific embodiments, the reaction temperature may be 140°C to 170°C. The reaction pressure may be 0.8 MPa to 1.2 MPa. The reaction time may be 2 hours to 15 hours (e.g., 2 hours, 3 hours, 4 hours, 5 hours, 6 hours, 7 hours, 8 hours, 9 hours, 10 hours, 11 hours, 12 hours, 13 hours, 14 hours, or 15 hours). Optimizing the reaction temperature, pressure, and time can help improve the reaction conversion rate.

[0055] In certain embodiments, the non-aqueous solvent comprises one or more of methylene chloride, dichloroethane, ethyl acetate, acetonitrile, ether, ethylene glycol dimethyl ether, and dimethyl carbonate. Of course, the non-aqueous solvent of the present invention can also be other commonly used non-aqueous solvents, and the present invention is not particularly limited to the non-aqueous solvent. In order to ensure that the reaction is carried out under anhydrous conditions, the moisture content of the non-aqueous solvent is required to be below 50ppm. The lower the moisture content, the less the hydrolysis of reaction raw materials and product, the higher the conversion rate of the reaction, and the higher the yield of the product.

[0056] In some specific embodiments, the water content of the non-aqueous solvent may be less than 50 ppm, less than 45 ppm, less than 40 ppm, less than 35 ppm, less than 30 ppm, less than 25 ppm, less than 20 ppm, less than 15 ppm, less than 10 ppm, or less than 5 ppm.

[0057] In some embodiments, the reaction is carried out in an anhydrous atmosphere. Prior to initiating the reaction, a protective gas may be introduced into the reaction vessel for purging to maintain an anhydrous atmosphere. The reaction vessel may include an autoclave, etc. The protective gas may include nitrogen, argon, etc.

[0058] In some embodiments, reacting a trialkylsilicon alkoxide with a phosphorus oxyhalide in a non-aqueous solvent comprises: dissolving the trialkylsilicon alkoxide in the non-aqueous solvent to obtain a mixed solution; and adding the phosphorus oxyhalide to the mixed solution. Phosphorus oxytrifluoride is a gas, while phosphorus oxychloride and phosphorus oxybromide are liquids. When phosphorus oxyfluoride is used, phosphorus oxyfluoride gas may be introduced into the mixed solution.

[0059] In some embodiments, after the reaction is completed, the method further comprises post-processing the resulting reaction solution. The post-processing comprises filtration and vacuum distillation. The completion of the reaction can be determined by monitoring the change in the product content in the reaction system. After the reaction is completed, the product content in the reaction system remains unchanged. After the reaction is completed, it is necessary to first release the pressure. After the pressure is released, the reaction mixture can be filtered to remove the precipitate and the filtrate can be collected. The filtrate is subjected to vacuum distillation to remove the solvent. Different solvents have different boiling points and corresponding distillation conditions are also different. Those skilled in the art can select appropriate distillation conditions based on the non-aqueous solvent used. The post-processing of the present invention is simple, and high-purity products can be obtained by only vacuum distillation.

[0060] In some embodiments, the temperature of the vacuum distillation may be 10° C. to 180° C. The pressure of the vacuum distillation may be -0.098 MPa to 0.098 MPa.

[0061] In some specific embodiments, the temperature of the vacuum distillation may be 10° C., 20° C., 40° C., 60° C., 80° C., 100° C., 120° C., 140° C., 160° C., or 180° C. The pressure of the vacuum distillation may be -0.098 MPa, -0.095 MPa, -0.09 MPa, 0.01 MPa, 0.02 MPa, 0.03 MPa, 0.04 MPa, 0.05 MPa, 0.06 MPa, 0.07 MPa, 0.08 MPa, 0.09 MPa, or 0.098 MPa.

[0062] Preferably, the temperature of the vacuum distillation may be 150° C. to 170° C. The pressure of the vacuum distillation may be -0.098 MPa to -0.09 MPa.

[0063] Below, the scheme of the present invention will be explained in conjunction with embodiment.It will be understood by those skilled in the art that the following examples are only used to illustrate the present invention and should not be regarded as limiting the scope of the present invention.In the embodiment, if specific technology or conditions are not indicated, the technology or conditions described in the literature in this area or the product instructions are used.The reagents or instruments used are not indicated by the manufacturer, and are all conventional products that can be obtained by commercial purchase.

[0064] Example 1

[0065] Nitrogen was purged into the autoclave to maintain a nitrogen-free atmosphere. Sodium trimethylsiliconate (CAS: 18027-10-6) (34.775 g, 0.310 mol) and a non-aqueous solvent, dichloromethane (102.66 g), were then added. The water content of the dichloromethane was 30 ppm. After stirring and dissolving, POF3 gas (10.397 g, 0.10 mol) was introduced. The molar ratio of sodium trimethylsiliconate to POF3 was 3.1:1. The reaction temperature was controlled at 155°C and the pressure was 1.0 MPa. After a reaction time of 6 h, the product content in the reaction mixture did not change. The reaction was stopped, the pressure was released, and the precipitate was removed by filtration. The resulting filtrate was freed of solvent at 20°C and -0.095 MPa. The temperature was then raised to 160°C, and the product was collected to obtain 26.74 g of tris(trimethylsilyl)phosphate with a gas chromatographic purity of 99% and a yield of 85%. The phosphorus spectrum of the product was as follows: Figure 1 shown.

[0066] Example 2

[0067] Tris(trimethylsilyl)phosphate was prepared according to the method described in Example 1, except that lithium trimethylsilanol (CAS: 2004-14-0) was used instead of sodium trimethylsilanol. The amount of lithium trimethylsilanol used is shown in Table 1. The gas chromatographic purity and yield of the product are also shown in Table 1.

[0068] Example 3

[0069] Tris(trimethylsilyl)phosphate was prepared according to the method described in Example 1, except that potassium trimethylsilanol (CAS: 10519-96-7) was used instead of sodium trimethylsilanol. The amount of potassium trimethylsilanol used is shown in Table 1. The gas chromatographic purity and yield of the product are shown in Table 1.

[0070] Example 4

[0071] Tris(trimethylsilyl)phosphate was prepared according to the method described in Example 1, except that phosphorus oxychloride was used instead of POF3. The amount of phosphorus oxychloride used is shown in Table 1. The gas chromatographic purity and yield of the product are shown in Table 1.

[0072] Example 5

[0073] Tris(trimethylsilyl)phosphate was prepared according to the method described in Example 1, except that phosphorus oxybromide was used instead of POF3. The amount of phosphorus oxybromide used is shown in Table 1. The gas chromatographic purity and yield of the product are shown in Table 1.

[0074] Example 6

[0075] Tris(triethylsilyl)phosphate was prepared according to the method described in Example 1, except that potassium triethylsilanol (CAS: 25706-33-6) was used instead of sodium trimethylsilanol. The amount of potassium triethylsilanol used is shown in Table 1. The gas chromatographic purity and yield of the product are shown in Table 1. The phosphorus spectrum of the product is shown in Table 1. Figure 2 shown.

[0076] Example 7

[0077] Tris(triethylsilyl)phosphate was prepared according to the method described in Example 6, except that phosphorus oxychloride was used instead of POF3. The amount of phosphorus oxychloride used is shown in Table 1. The gas chromatographic purity and yield of the product are shown in Table 1.

[0078] Example 8

[0079] Tris(triethylsilyl)phosphate was prepared according to the method described in Example 6, except that phosphorus oxybromide was used instead of POF3. The amount of phosphorus oxybromide used is shown in Table 1. The gas chromatographic purity and yield of the product are shown in Table 1.

[0080] Example 9

[0081] Tris(trimethylsilyl)phosphate was prepared according to the method described in Example 1, except that the reaction temperature was 140° C. The gas chromatographic purity and yield of the product are shown in Table 1.

[0082] Example 10

[0083] Tris(trimethylsilyl)phosphate was prepared according to the method described in Example 1, except that the reaction temperature was 170° C. The gas chromatographic purity and yield of the product are shown in Table 1.

[0084] Example 11

[0085] Tris(trimethylsilyl)phosphate was prepared according to the method described in Example 1, except that the reaction temperature was 100° C. The gas chromatographic purity and yield of the product are shown in Table 1.

[0086] Example 12

[0087] Tris(trimethylsilyl)phosphate was prepared according to the method described in Example 1, except that the reaction temperature was 200° C. The gas chromatographic purity and yield of the product are shown in Table 1.

[0088] Example 13

[0089] Tris(trimethylsilyl)phosphate was prepared according to the method described in Example 1, except that the reaction pressure was 0.8 MPa. The gas chromatographic purity and yield of the product are shown in Table 1.

[0090] Example 14

[0091] Tris(trimethylsilyl)phosphate was prepared according to the method described in Example 1, except that the reaction pressure was 1.2 MPa. The gas chromatographic purity and yield of the product are shown in Table 1.

[0092] Example 15

[0093] Tris(trimethylsilyl)phosphate was prepared according to the method described in Example 1, except that the reaction pressure was 0.6 MPa. The gas chromatographic purity and yield of the product are shown in Table 1.

[0094] Example 16

[0095] Tris(trimethylsilyl)phosphate was prepared according to the method described in Example 1, except that the reaction pressure was 1.5 MPa. The gas chromatographic purity and yield of the product are shown in Table 1.

[0096] Example 17

[0097] Tris(trimethylsilyl)phosphate was prepared according to the method described in Example 1, except that the molar ratio of trialkylsilanol salt to phosphorus oxyhalide was 3.2:1. The gas chromatographic purity and yield of the product are shown in Table 1.

[0098] Example 18

[0099] Tris(trimethylsilyl)phosphate was prepared according to the method described in Example 1, except that the water content of dichloromethane was 100 ppm. The gas chromatographic purity and yield of the product are shown in Table 1.

[0100] Example 19

[0101] Tris(trimethylsilyl)phosphate was prepared according to the method described in Example 1, except that nitrogen was not introduced into the autoclave for purging.

[0102] Comparative Example 1

[0103] Tris(trimethylsilyl)phosphate was prepared according to the method described in Example 1, except that water was used instead of dichloromethane. The gas chromatographic purity and yield of the product are shown in Table 1.

[0104] Comparative Example 2

[0105] Tris(trimethylsilyl)phosphate was prepared according to the method described in Example 1, except that the reaction temperature was 80° C. The gas chromatographic purity and yield of the product are shown in Table 1.

[0106] Comparative Example 3

[0107] Tris(trimethylsilyl)phosphate was prepared according to the method described in Example 1, except that the reaction temperature was 220° C. The gas chromatographic purity and yield of the product are shown in Table 1.

[0108] Comparative Example 4

[0109] Tris(trimethylsilyl)phosphate was prepared according to the method described in Example 1, except that the reaction pressure was 0.4 MPa. The gas chromatographic purity and yield of the product are shown in Table 1.

[0110] Comparative Example 5

[0111] Tris(trimethylsilyl)phosphate was prepared according to the method described in Example 1, except that the reaction pressure was 1.7 MPa. The gas chromatographic purity and yield of the product are shown in Table 1.

[0112] Comparative Example 6

[0113] Tris(trimethylsilyl)phosphate was prepared according to the method described in Example 1, except that the molar ratio of trialkylsilicon alkoxide to phosphorus oxyhalide was 3.0:1. The gas chromatographic purity and yield of the product are shown in Table 1.

[0114] Comparative Example 7

[0115] Tris(trimethylsilyl)phosphate was prepared according to the method described in Example 1, except that the molar ratio of trialkylsilicon alkoxide to phosphorus oxyhalide was 3.5:1. The gas chromatographic purity and yield of the product are shown in Table 1.

[0116] Table 1

[0117]

[0118] Results and Discussion

[0119] By comparing Examples 1-19 with Comparative Example 1, it can be seen that the reaction system for preparing tri(trialkylsilane)phosphate of the present invention has strict requirements on moisture content. The presence of excessive moisture will cause the raw materials and target products to decompose and generate by-products, thereby reducing the yield and purity of the product.

[0120] By comparing Example 1 with Comparative Examples 2-3, it can be seen that too high or too low a reaction temperature is not conducive to the purity and yield of the product, especially the yield of the product.

[0121] By comparing Example 1, Example 17 and Comparative Examples 4-5, it can be seen that too high or too low reaction pressure is not conducive to the purity and yield of the product, especially the yield of the product.

[0122] By comparing Example 1 with Comparative Examples 6-7, it can be seen that a too high or too low molar ratio of trialkylsilicon alkoxide to phosphorus oxyhalide is detrimental to the purity and yield of the product, especially the yield of the product.

[0123] By comparing Example 1 with Examples 4-5, it can be seen that in Example 4-5, phosphorus oxychloride and phosphorus oxybromide are used as raw materials to prepare tris(trialkylsilane) phosphate, and the product yield is reduced. The possible reason is that the reactivity of phosphorus oxychloride and phosphorus oxybromide is reduced compared with phosphorus oxyfluoride.

[0124] By comparing Example 1 with Examples 9-12, it can be seen that the reaction temperature affects the yield and purity of the product. Controlling the reaction temperature within the range of 140°C-170°C is more conducive to improving the yield and purity.

[0125] By comparing Example 1 with Examples 13-16, it can be seen that the reaction pressure affects the yield and purity of the product. Controlling the reaction pressure within the range of 0.8 MPa-1.2 MPa is more conducive to improving the yield and purity.

[0126] By comparing Example 1 with Examples 18-19, it can be seen that the moisture in the reaction raw materials and the reaction atmosphere will reduce the purity of the product, especially the yield, and the moisture content of the reaction system needs to be strictly controlled.

[0127] In summary, the present invention provides a novel method for preparing tris(trialkylsilane)phosphate. The method uses trialkylsilanol salt and trihalogenated phosphorus as reaction raw materials, and reacts under heating and pressure to produce tris(trialkylsilane)phosphate. The process is simple, the reaction conversion rate is high, the product purity is high, and the post-processing is simple.

[0128] In the description of this specification, reference to the terms "one embodiment," "some embodiments," "example," "specific example," or "some examples" means that the specific features, structures, materials, or characteristics described in conjunction with the embodiment or example are included in at least one embodiment or example of the present invention. In this specification, the schematic representations of the above terms do not necessarily refer to the same embodiment or example. Moreover, the specific features, structures, materials, or characteristics described may be combined in any appropriate manner in any one or more embodiments or examples. In addition, those skilled in the art may combine and combine different embodiments or examples described in this specification, as well as features of different embodiments or examples, unless they are mutually inconsistent.

[0129] Although the embodiments of the present invention have been shown and described above, it will be understood that the above embodiments are illustrative and are not to be construed as limitations on the present invention. A person skilled in the art may change, modify, replace and modify the above embodiments within the scope of the present invention.

Claims

1. A method for preparing tris(trialkylsilane)phosphate, characterized in that: The following steps are involved: At 100°C-200°C and 0.6MPa-1.5MPa, a trialkylsilicon alkoxide represented by Chemical Formula 1 and a trihalogenated phosphorus represented by Chemical Formula 2 are reacted in a non-aqueous solvent at a molar ratio of (3.05-3.2):1 to generate tris(trialkylsilane)phosphate. Chemical formula 1 Chemical formula 2 in, R is selected from C1-C6 alkyl; M is selected from any one of lithium, sodium and potassium; X is selected from any one of fluorine, chlorine and bromine, The non-aqueous solvent is one or more of dichloromethane, dichloroethane, ethyl acetate, acetonitrile, diethyl ether, ethylene glycol dimethyl ether, and dimethyl carbonate.

2. The method according to claim 1, characterized in that R is selected from C1-C4 alkyl.

3. The method according to claim 1, characterized in that R is selected from any one of methyl and ethyl.

4. The method according to claim 1, wherein X is selected from fluorine.

5. The method according to claim 1, wherein The reaction temperature is 140°C-170°C, the reaction pressure is 0.8MPa-1.2MPa, and the reaction time is 2h-15h.

6. The method according to claim 1, characterized in that The water content of the non-aqueous solvent is below 50 ppm.

7. The method according to claim 1, characterized in that The reaction was carried out in an anhydrous atmosphere.

8. The method according to claim 1, characterized in that After the reaction is completed, the method further comprises post-processing the obtained reaction solution; The post-processing includes filtration and vacuum distillation; The temperature of the vacuum distillation is 10°C-180°C, and the pressure is -0.098MPa ~ 0.098MPa.

9. The method according to claim 1, characterized in that The method of reacting trialkyl silicon alkoxide with phosphorus oxyhalide in a non-aqueous solvent comprises: dissolving the trialkyl silicon alkoxide in the non-aqueous solvent to obtain a mixed solution; and adding the phosphorus oxyhalide into the mixed solution.

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